Method of increasing the curl, filling power, etc., of land fowl feathers with zirconium sulfate and product produced thereby



United States Patent METHOD OF INCREASING THE CURL, FILLING POWER, ETC., OF LAND FOWL FEATHERS WITH ZIRCONIUM SULFATE AND PRODUCT PRO- DUCED THEREBY Varsenig Z. Pasternak and Robert M. Lollar, Cincinnati, Ohio, assignors to the United States of America as represented by the Secretary of the Army No Drawing. Application April 23, 1957 Serial No. 654,616

8 Claims. (01. 894.1)

This invention relates to a method of treating land fowl feathers, especially chicken feathers, to increase their filling power and resiliency, and to impart permanent curliness and water repellency, thereby making such feathers an acceptable. substitute for the standard'down and feather mixture now in wide use for sleeping bags,

entitled Investigation of Methods for Determining the Filling Power of Feathers. See also the Sinski et a1. Patent No. 2,706,910, dated April 26, 1955. Ordinarily, chicken feathers have a filling power of 1.8 to 2.1 cm., while the 40/60 down-feather mixture has a filling power of 5.3 to 5.9 cm.

The term feathers as used herein includes whole land fowl feathers of the desired size range, crushed (commercial curled) land fowl feathers, land fowl feather fibers, stripped land fowl feathers, and mixtures of these.

In' the preferred procedure, the feathers, if not known to be entirely free from blood, are first soaked for about ten minutes in a water solution of a commercial blood solubilizer, such as Coagusol (a mixture of sodium hexametaphosphate and alcohol sulfate). After the soaking, the solution is drained from the feathers and the feathers are then laundered or dry cleaned. In laundering, preferably adetergent such as Tergitol NPX (alkyl phenyl ether of polyethylene glycol) is used (0.25% water solution at 110-125 F.). Other non-ionic detergents have been found to be satisfactory. In general, the nonionic type of detergents should be used to obviate any action on the protein of the feathers. Laundering con tinues for about twenty minutes, then the solution is removed from the feathers by centrifuging or wringing. While a number of well-known dry cleaning solutions could be used to clean the feathers, laundering is preferred because it is less expensive. Both laundering and dry cleaning may take place in the same vessel or container that is used during the blood-s'olubilizing step. Of course, if the feathers as initially received are perfectly clean, the soaking and washing or dry cleaning may be omitted.

If the feathers are from immature chickens, the damp feathers from the described laundering or dry cleaning operation are placed in a 1% water solution of trisodium phosphate Na PO .12H O at 43 -49 C. for about ten minutes. If feathers from mature chickens are being processed, the phosphate treatment period is increased to about thirty minutes. This mild alkaline treatment of I 2 the feathers is believed to alter the stability of the feathers by modification of the cystine linkages in the keratin. This step is important because it materially increases the curliness of the feathers andit curls naturally uncurly mature feathers, thereby to increase the bulk value of the final feather product. Other suitably buffered alkaline solutions, for example, sodium carbonate or borax, may be used in lieu of the phosphate solution mentioned above, but in all cases the time of the treatment must be less for immature feathers to avoid excessive degradation. Trisodium phosphate is preferred because of its quicker action due to a higher pH. It is believed that the higher concentration of cystine linkages in mature feathers enables them to resist the action of the alkaline solution for a longer period.

The data from three successful laboratory runs at The Tanners Council Research Laboratory, University of Cincinnati, will now be given:

NORMAL ZIRCONIUM SULFATE TREATMENT A batch of 67 grams of chicken feathers was first treated with trisodium phosphate as described above, then the feathers were rinsed. The damp feathers were immersed in a bath of 1 liter of 6% normal zirconium sulfate water solution, Zr(SO .4H O with the pH controlled as follows:

1.6 for thirty minutes ;3.23.3 for minutes 4.2 for ten minutes Increase in the pH was effected by adding Na CO solution. The temperature varied from 4047 C. Then the feathers were removed from the solution, rinsed for thirty minutes, dried and cured. The filling power was 6.1 cm. The product of this process is always white feathers.

BASIC ZIRCONIUM SULFATE A batch of 67 grams of chicken feathers was first treated with trisodium phosphate as described above, then the feathers were rinsed in water. The damp feathers were immersed in 1 liters of a 3% solution'of basic zirconium sulfate for three hours at 42-46 C. at these pH levels:

2.4 for forty minutes 2.7 for twenty-five minutes 3.2 for eighty-five minutes 4.3 for thirty minutes The increase in the pH was effected by adding Na CO solution. Basic zirconium sulfate, which is commercially sold under the trademark Zircotan N, has the chemical formula Zr(OH) SO .N-a SO At the end of the treatment thefeathers were removed, rinsed for'thii'ty minutes, then dried and relaxed. The filling power was 6.1 cm. The product is always white feathers.

BROMOACETIC OR CHLO-ROAOETIC ACID PLUS .BASIC ZIRCONIUM SULFATE The damp feathers were treated with basic zirconium sulfate for three hours at 42 -46 C., the pH being 3.2-

3.3; however, for the last ten minutes of the treatment A the pH was raised to 4.7 by adding Na CO solution. Then the feathers were removed, rinsed for thirty minutes,

Patented Feb. 23, 1960 dried and cured. The filling power was 6.2 cm. Here again the product is always white feathers.

Practically the same procedure is followed when employing chloroacetic acid (monochloroacetic acid) CH C-LCOOH in lieu of bromoacetic acid; but the bath of 1500 ml. will use 2.4% chloroacetic acid for the same pH and at the same temperature range.

The use of sodium carbonate or its equivalent to raise the pH is apparently an important step, as the following table indicates.

Table SHOWING EFFECT OF RAISING THE pH IN BASIC ZIRCONIUM SULFATE TREATMENT OF CHICKEN When no bromoacetic acid was used, the filling power under the same test conditions dropped to 5.7 cm. (runs Nos. 228 and 242). On the other hand, when working with well-washed immature feathers of White Rock chickens and using 3% basic zirconium sulfate at pH 2.6 to 3.3, the filling power was exactly the same, whether bromoacetic acid was used or omitted (runs Nos. 259 and 267).

Having described our invention, we claim:

1. A method of treating land fowl feathers to enhance their filling power, which comprises modifying the cystine linkage of the keratin of said land fowl feathers by immersing said feathers in an aqueous alkaline solution until their curliness is increased, rinsing said feathers, then placing the feathers in an aqueous sulfate solution of a member of the group consisting of normal zirconium sulfate and basic zirconium sulfate, the pH of said aqueous sulfate solution being about 1.6-3.3 and the temperature of said aqueous sulfate solution being about 40- 47 C., raising the pH of the said aqueous sulfate solution to about 4.2-4.7, keeping said feathers in said aqueous sulfate solution until their filling power is substantially increased, then removing the feathers from said aqueous sulfate solution and rinsing and drying them.

2. The method according to claim 1, wherein said land fowl feathers are kept in said last-mentioned solution for about three hours.

31 The method according to claim 1, wherein said aqueous alkaline solution is an approximately 1% solution of trisodium phosphate having a temperature of about 43 -49 C., said immersion having a duration of about -30 minutes.

4. A method of treating land fowl feathers to enhance their filling power, which comprises modifying the cystine linkage of the keratin of said land fowl feathers by immersing said feathers in an aqueous alkaline solution until their curliness is increased, rinsing said feathers, then placing the land fowl feathers in a bath ofan ap proximately 6% water solution of normal zirconium sul- 6 fate at a pH of about 1.6 for about thirty minutes, increasing the pH to about 3.2-3.3 for about 140 minutes,

4 and further increasing the pH to about 4.2 for about ten minutes, then removing the feathers from said solution, and rinsing and drying them.

5. A method of treating land fowl feathers to enhance their filling power which comprises modifying the cystine linkage of the keratin of said land fowl feathers by immersing said feathers in anaqueous alkaline solution until their curliness is increased, rinsing said feathers, then immersing the land fowl feathers in an about 3% aqueous solution of basic zirconium sulfate for about three hours at about 42-46 C., the pH being about 2.4 for about forty minutes, then raising it to about 2.7 for about twenty-five minutes, then raising it further to about 3.2 for about eighty-five minutes, and finally raising it to about 4.3 for about thirty minutes, then removing the feathers from said solution, and rinsing and drying them.

6. A method of treating land fowl feathers to enhance their filling power, which comprises modifying the cystine linkage of the keratin of said land fowl feathers by immersing said feathers in an aqueous alkaline solution until their curliness is increased, rinsing said feathers, then immersing the land fowl feathers in a bath of an about 3.5% water solution of bromoacetic acid for about twenty minutes, then raising the pH to about 9.2-9.4, and continuing the treatment for about two hours at about 42-46 C., then removing the feathers from said bath and rinsing them with water, then immersing the feathers in an aqueous bath of basic zirconium sulfate for about three hours at about 42-46 C., the pH being about 3.2-3.3 for all but the last approximately ten minutes when it is raised to about 4.7, then removing the feathers from said zirconium bath, and rinsing and drying them.

7. A method of treating land fowl feathers to enhance their filling power which comprises modifying the cystine linkage of the keratin of said land fowl feathers by immersing said feathers in an aqueous alkaline solution until their curliness is increased, rinsing said feathers, then immersing the land fowl feathers in a bath of an about 2.4% water solution of chloroacetic acid for about twenty minutes, then'r-aising the'pH to about 9.2-9.4 and continuing the treatment for about two hours at about 4246 C. then removing the feathers from said bath and rinsing them with water, then immersing the feathers in an aqueous bath of basic zirconium sulfate for about three hours at about 42-46 C., the pH being about 3.2 to 3.3 for all but the last approximately ten minutes when it is raised to about 4.7, then removing the feathers from said zirconium bath, and rinsing and drying them.

8. The product produced by the method of claim 1.

References Cited in the file of this patent UNITED STATES PATENTS 2,129,219 Koga Sept. 6, 1938 2,184,147 Lowe Dec. 19, 1939 2,261,094 Speakman Oct. 28, 1941 2,294,384 Champion Sept. 1, 1942 2,426,861 Comolli Sept. 2, 1947 2,567,184 Corwin Sept. 11, 1951 2,805,913 Frederick Sept. 10, 1957 2,805,914 Frederick Sept. 10, 1957 OTHER REFERENCES Speakman: I. of the Soc. of Dyers and Colourists, September 1936, pp. 335-346.

Speakman: I. of the Sec. of Dyers and Colourists, June 1937, pp. 236-242.

UNITED STATES PAI'ENT OFFICE CERTIFICATE OF CORRECTION atent No, 2,926,061 February 23, 1960 Varsenig Z. Pasternak et al. I

It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction and "that thesaid Letters Patent should read as corrected below.

Column 3, line 52, for last-mentioned' read aqueous sulfate Signed and sealed this 2nd day of August 1960,

SEAL) Lttest: I LARL H, AXLINE ROBERT C. WATSON Ittesting Officer Commissioner of Patents 

1. A METHOD OF TREATING LAND FOWL FEATHERS TO ENHANCE THEIR FILLING POWER, WHICH COMPRISES MODIFYING THE CYSTINE LINKAGE OF THE KERATIN OF SAID LAND FOWL FEATHERS BY IMMERSING SAID FEATHERS IN AN AQUEOUS ALKALINE SOLUTION UNTIL THEIR CURLINESS IS INCREASED, RINSING SAID FEATHERS, THEN PLACING THE FEATHERS IN AN AQUEOUS SULFATE SOLUTION OF A MEMBER OF THE GROUP CONSISTING OF NORMAL ZIRCONIUM SULFATE AND BASIC ZIRCONIUM SULFATE, THE PH OF SAID AQUEOUS SULFATE SOLUTION BEING ABOUT 1.6-3.3 AND THE TEMPERATURE OF SAID AQUEOUS SULFATE SOLUTION BEING ABOUT 40*47* C., RAISING THE PH OF THE SAID AQUEOUS SULFATE SOLUTION TO ABOUT 4.2-4.7, KEEPING SAID FEATHERS IN SAID AQUEOUS SULFATE SOLUTION UNTIL THEIR FILLING POWER IS SUBSTANTIALLY INCREASED, THEN REMOVING THE FEATHERS FROM SAID AQUEOUS SULFATE SOLUTION AND RINSING AND DRYING THEM. 